反应详情

2-Ethyl-4-(1,1,1,2,3,3,3-heptafluoropropan-2-yl)-6-methylaniline (0.50 g) and pyridine (0.20 g) were dissolved in tetrahydrofuran (10 ml). To the solution, 4-(chloromethyl)benzoyl chloride (0.33 g) and 4-dimethylaminopyridine (0.02 g) were added and the mixture was refluxed under heating for 3 hours. After adjusting to room temperature, the reaction solution was diluted with water and extracted twice with ethyl acetate. The organic phases were combined, washed with 2N hydrochloric acid and dried over Mg(SO4). After filtering off the drying agent, the solvent was distilled off under reduced pressure to obtain a crude product. The crude product was washed with hexane to obtain 4-(chloro methyl)-N-[2-ethyl-4-(1,1,1,2,3,3,3-heptafluoro-propan-2-yl)-6-methylphenyl]benzamide (0.62 g, yield 74%).

1. temperaturethe mixture was refluxed
2. temperatureunder heating for 3 hours
3. customAfter adjusting to room temperature
4. extractionextracted twice with ethyl acetate
5. washwashed with 2N hydrochloric acid
6. dry with materialdried over Mg(SO4)
7. filtrationAfter filtering off the drying agent
8. distillationthe solvent was distilled off under reduced pressure
9. customto obtain a crude product
10. washThe crude product was washed with hexane